Direct-write liquid phase transformations with a scanning transmission electron microscope

Unocic, Raymond R.; Lupini, Andrew R.; Borisevich, Albina Y.; Cullen, David A.; Kalinin, Sergei V.; Jesse, Stephen

doi:10.1039/C6NR04994J

Direct-write liquid phase transformations with a scanning transmission electron microscope

Journal Article · Wed Aug 03 00:00:00 EDT 2016 · Nanoscale

DOI:https://doi.org/10.1039/C6NR04994J· OSTI ID:1333640

Unocic, Raymond R. ^[1]; Lupini, Andrew R. ^[1]; Borisevich, Albina Y. ^[1]; Cullen, David A. ^[1]; Kalinin, Sergei V. ^[1]; Jesse, Stephen ^[1]

Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

The highly energetic electron beam from a scanning transmission electron microscope (STEM) can induce local changes in the state of matter, ranging from local knock-out and atomic movement, to amorphization/crystallization, and chemical/electrochemical reactions occuring at localized liquid-solid and gas-solid interfaces. To date, fundamental studies of e-beam induced phenomena and practical applications have been limited by conventional e-beam rastering modes that allow only for uniform e-beam exposures. Here we develop an automated liquid phase nanolithography method that is capable of directly writing nanometer scaled features within silicon nitride encapsulated liquid cells. An external beam control system, connected to the scan coils of an aberration-corrected STEM, is used to precisely control the position, dwell time, and scan velocity of a sub-nanometer STEM probe. Site-specific locations in a sealed liquid cell containing an aqueous solution of H₂PdCl₄ are irradiated to controllably deposit palladium onto silicon nitride membranes. We determine the threshold electron dose required for the radiolytic deposition of metallic palladium, explore the influence of electron dose on the feature size and morphology of nanolithographically patterned nanostructures, and propose a feedback-controlled monitoring method for active control of the nanofabricated structures through STEM detector signal monitoring. As a result, this approach enables both fundamental studies of electron beam induced interactions with matter, as well as opens a pathway to fabricate nanostructures with tailored architectures and chemistries via shape-controlled nanolithographic patterning from liquid phase precursors.

View Accepted Manuscript (DOE)

Research Organization:: Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States). Center for Nanophase Materials Sciences (CNMS)

Sponsoring Organization:: USDOE Office of Science (SC)

Grant/Contract Number:: AC05-00OR22725

OSTI ID:: 1333640

Journal Information:: Nanoscale, Journal Name: Nanoscale Journal Issue: 34 Vol. 8; ISSN NANOHL; ISSN 2040-3364

Publisher:: Royal Society of ChemistryCopyright Statement

Country of Publication:: United States

Language:: English

References (35)

Writing Silica Structures in Liquid with Scanning Transmission Electron Microscopy van de Put, Marcel W. P.; Carcouët, Camille C. M. C.; Bomans, Paul H. H. Small, Vol. 11, Issue 5 https://doi.org/10.1002/smll.201400913	journal	September 2014
Atomic-Level Sculpting of Crystalline Oxides: Toward Bulk Nanofabrication with Single Atomic Plane Precision Jesse, Stephen; He, Qian; Lupini, Andrew R. Small, Vol. 11, Issue 44 https://doi.org/10.1002/smll.201502048	journal	October 2015
Impact of Membrane-Induced Particle Immobilization on Seeded Growth Monitored by In Situ Liquid Scanning Transmission Electron Microscopy Weiner, Rebecca G.; Chen, Dennis P.; Unocic, Raymond R. Small, Vol. 12, Issue 20 https://doi.org/10.1002/smll.201502974	journal	April 2016
Microfluidic System for Transmission Electron Microscopy Ring, Elisabeth A.; de Jonge, Niels Microscopy and Microanalysis, Vol. 16, Issue 5 https://doi.org/10.1017/S1431927610093669	journal	August 2010
The Probe Profile and Lateral Resolution of Scanning Transmission Electron Microscopy of Thick Specimens Demers, Hendrix; Ramachandra, Ranjan; Drouin, Dominique Microscopy and Microanalysis, Vol. 18, Issue 3 https://doi.org/10.1017/S1431927612000232	journal	May 2012
Gaining Control over Radiolytic Synthesis of Uniform Sub-3-nanometer Palladium Nanoparticles: Use of Aromatic Liquids in the Electron Microscope Abellan, Patricia; Parent, Lucas R.; Al Hasan, Naila Langmuir, Vol. 32, Issue 6 https://doi.org/10.1021/acs.langmuir.5b04200	journal	February 2016
Electron–Water Interactions and Implications for Liquid Cell Electron Microscopy Schneider, Nicholas M.; Norton, Michael M.; Mendel, Brian J. The Journal of Physical Chemistry C, Vol. 118, Issue 38 https://doi.org/10.1021/jp507400n	journal	September 2014
Controlled Growth of Nanoparticles from Solution with In Situ Liquid Transmission Electron Microscopy Evans, James E.; Jungjohann, Katherine L.; Browning, Nigel D. Nano Letters, Vol. 11, Issue 7 https://doi.org/10.1021/nl201166k	journal	July 2011
Mapping Irreversible Electrochemical Processes on the Nanoscale: Ionic Phenomena in Li Ion Conductive Glass Ceramics Arruda, Thomas M.; Kumar, Amit; Kalinin, Sergei V. Nano Letters, Vol. 11, Issue 10 https://doi.org/10.1021/nl202039v	journal	October 2011
Probing Local Ionic Dynamics in Functional Oxides at the Nanoscale Strelcov, Evgheni; Kim, Yunseok; Jesse, Stephen Nano Letters, Vol. 13, Issue 8 https://doi.org/10.1021/nl400780d	journal	July 2013
In Situ Liquid Cell Electron Microscopy of the Solution Growth of Au–Pd Core–Shell Nanostructures Jungjohann, K. L.; Bliznakov, S.; Sutter, P. W. Nano Letters, Vol. 13, Issue 6 https://doi.org/10.1021/nl4014277	journal	May 2013
Bubble and Pattern Formation in Liquid Induced by an Electron Beam Grogan, Joseph M.; Schneider, Nicholas M.; Ross, Frances M. Nano Letters, Vol. 14, Issue 1 https://doi.org/10.1021/nl404169a	journal	December 2013
Direct Observation of Aggregative Nanoparticle Growth: Kinetic Modeling of the Size Distribution and Growth Rate Woehl, Taylor J.; Park, Chiwoo; Evans, James E. Nano Letters, Vol. 14, Issue 1 https://doi.org/10.1021/nl4043328	journal	December 2013
In situ Study of Oxidative Etching of Palladium Nanocrystals by Liquid Cell Electron Microscopy Jiang, Yingying; Zhu, Guomin; Lin, Fang Nano Letters, Vol. 14, Issue 7 https://doi.org/10.1021/nl500670q	journal	June 2014
Determining the Resolution Limits of Electron-Beam Lithography: Direct Measurement of the Point-Spread Function Manfrinato, Vitor R.; Wen, Jianguo; Zhang, Lihua Nano Letters, Vol. 14, Issue 8 https://doi.org/10.1021/nl5013773	journal	June 2014
Direct in Situ Observation of Nanoparticle Synthesis in a Liquid Crystal Surfactant Template Parent, Lucas R.; Robinson, David B.; Woehl, Taylor J. ACS Nano, Vol. 6, Issue 4 https://doi.org/10.1021/nn300671g	journal	March 2012
Direct in Situ Determination of the Mechanisms Controlling Nanoparticle Nucleation and Growth Woehl, Taylor J.; Evans, James E.; Arslan, Ilke ACS Nano, Vol. 6, Issue 10 https://doi.org/10.1021/nn303371y	journal	September 2012
Atom-by-atom structural and chemical analysis by annular dark-field electron microscopy Krivanek, Ondrej L.; Chisholm, Matthew F.; Nicolosi, Valeria Nature, Vol. 464, Issue 7288 https://doi.org/10.1038/nature08879	journal	March 2010
Direct visualization of reversible dynamics in a Si6 cluster embedded in a graphene pore Lee, Jaekwang; Zhou, Wu; Pennycook, Stephen J. Nature Communications, Vol. 4, Issue 1 https://doi.org/10.1038/ncomms2671	journal	April 2013
Electron microscopy of specimens in liquid de Jonge, Niels; Ross, Frances M. Nature Nanotechnology, Vol. 6, Issue 11, p. 695-704 https://doi.org/10.1038/nnano.2011.161	journal	October 2011
Flexible metallic nanowires with self-adaptive contacts to semiconducting transition-metal dichalcogenide monolayers Lin, Junhao; Cretu, Ovidiu; Zhou, Wu Nature Nanotechnology, Vol. 9, Issue 6 https://doi.org/10.1038/nnano.2014.81	journal	April 2014
Factors influencing quantitative liquid (scanning) transmission electron microscopy Abellan, P.; Woehl, T. J.; Parent, L. R. Chem. Commun., Vol. 50, Issue 38 https://doi.org/10.1039/C3CC48479C	journal	January 2014
Substrate effects on the electron-beam-induced deposition of platinum from a liquid precursor Donev, Eugenii U.; Schardein, Gregory; Wright, John C. Nanoscale, Vol. 3, Issue 7 https://doi.org/10.1039/c1nr10026b	journal	January 2011
Intrinsic single-domain switching in ferroelectric materials on a nearly ideal surface Kalinin, S. V.; Rodriguez, B. J.; Jesse, S. Proceedings of the National Academy of Sciences, Vol. 104, Issue 51 https://doi.org/10.1073/pnas.0709316104	journal	December 2007
Nanoscale ferroelectrics: processing, characterization and future trends Gruverman, A.; Kholkin, A. Reports on Progress in Physics, Vol. 69, Issue 8 https://doi.org/10.1088/0034-4885/69/8/R04	journal	July 2006
Creating pure nanostructures from electron-beam-induced deposition using purification techniques: a technology perspective Botman, A.; Mulders, J. J. L.; Hagen, C. W. Nanotechnology, Vol. 20, Issue 37 https://doi.org/10.1088/0957-4484/20/37/372001	journal	August 2009
The partially reversible formation of Li-metal particles on a solid Li electrolyte: applications toward nanobatteries Arruda, Thomas M.; Kumar, Amit; Kalinin, Sergei V. Nanotechnology, Vol. 23, Issue 32 https://doi.org/10.1088/0957-4484/23/32/325402	journal	July 2012
Electron beam induced deposition of silicon nanostructures from a liquid phase precursor Liu, Yin; Chen, Xin; Noh, Kyong Wook Nanotechnology, Vol. 23, Issue 38 https://doi.org/10.1088/0957-4484/23/38/385302	journal	September 2012
Direct Observation of Dopant Atom Diffusion in a Bulk Semiconductor Crystal Enhanced by a Large Size Mismatch Ishikawa, Ryo; Mishra, Rohan; Lupini, Andrew R. Physical Review Letters, Vol. 113, Issue 15 https://doi.org/10.1103/PhysRevLett.113.155501	journal	October 2014
Gas-assisted focused electron beam and ion beam processing and fabrication Utke, Ivo; Hoffmann, Patrik; Melngailis, John Journal of Vacuum Science & Technology B: Microelectronics and Nanometer Structures, Vol. 26, Issue 4 https://doi.org/10.1116/1.2955728	journal	January 2008
Atomic-Scale Chemical Imaging of Composition and Bonding by Aberration-Corrected Microscopy Muller, D. A.; Kourkoutis, L. F.; Murfitt, M. Science, Vol. 319, Issue 5866 https://doi.org/10.1126/science.1148820	journal	February 2008
Observation of Single Colloidal Platinum Nanocrystal Growth Trajectories Zheng, H.; Smith, R. K.; Jun, Y. -w. Science, Vol. 324, Issue 5932 https://doi.org/10.1126/science.1172104	journal	June 2009
Real-Time Imaging of Pt3Fe Nanorod Growth in Solution Liao, H. -G.; Cui, L.; Whitelam, S. Science, Vol. 336, Issue 6084 https://doi.org/10.1126/science.1219185	journal	May 2012
Facet development during platinum nanocube growth Liao, H. -G.; Zherebetskyy, D.; Xin, H. Science, Vol. 345, Issue 6199 https://doi.org/10.1126/science.1253149	journal	August 2014
Opportunities and challenges in liquid cell electron microscopy Ross, F. M. Science, Vol. 350, Issue 6267 https://doi.org/10.1126/science.aaa9886	journal	December 2015

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Resolution and aberration correction in liquid cell transmission electron microscopy de Jonge, Niels; Houben, Lothar; Dunin-Borkowski, Rafal E. Nature Reviews Materials, Vol. 4, Issue 1 https://doi.org/10.1038/s41578-018-0071-2	journal	December 2018
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Resolution and aberration correction in liquid cell transmission electron microscopy De Jonge, Niels; Houben, Lothar; Dunin-Borkowski, Rafal E. Universität des Saarlandes https://doi.org/10.22028/d291-29264	collection	January 2018

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